Classifications

• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B33/00—Silicon; Compounds thereof
  • C01B33/08—Compounds containing halogen
  • C01B33/107—Halogenated silanes
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
  • B01D3/14—Fractional distillation or use of a fractionation or rectification column
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B33/00—Silicon; Compounds thereof
  • C01B33/08—Compounds containing halogen
  • C01B33/107—Halogenated silanes
  • C01B33/10778—Purification

Definitions

• the present invention generally relates to a method of preparing pentachlorodisilane and, more specifically, to a method of preparing a purified reaction product comprising pentachlorodisilane with excellent yield and conversion and to the purified reaction produced formed thereby.
• Silane compounds are known in the art and utilized in diverse end use applications. For example, silane compounds may be utilized to prepare organopolysiloxanes, e.g. silicone polymers or resins. Alternatively, silane compounds are ubiquitously utilized in the electronics industry. For example, silane compounds are utilized to form thin films via deposition (e.g. chemical vapor deposition, atomic layer deposition, etc.). The thin films may comprise crystalline silicon, or silica (S1O2), depending on a selection of the silane compound utilized. Typically, such silane compounds include silicon- bonded hydrogen atoms (silicon hydride) and/or silicon-bonded halogen atoms.
• silane compounds include silicon- bonded hydrogen atoms (silicon hydride) and/or silicon-bonded halogen atoms.
• pentachlorodisilane is difficult to synthesize and expensive to otherwise obtain.
• one technique for synthesizing pentachlorodisilane involves oligomerizing a monosilane (e.g. S1CI4) in the presence of hydrogen (H2).
• Another technique involves cleaving silicon-silicon bonds in higher order silane compounds (e.g. tri- or higher order silane compounds).
• such techniques require significant energy and/or expensive starting reagents.
• the present invention provides a method of preparing pentachlorodisilane.
• the method comprises partially reducing hexachlorodisilane with a metal hydride compound to give a reaction product comprising pentachlorodisilane.
• the method further comprises purifying the reaction product to give a purified reaction product comprising the pentachlorodisilane.
• a method of preparing pentachlorodisilane is disclosed.
• the pentachlorodisilane is prepared in a purified reaction product and may be utilized in diverse end use applications.
• the pentachlorodisilane may be utilized as a starting component when preparing organopolysiloxanes, e.g. via cohydrolysis and co-condensation.
• the pentachlorodisilane may be utilized for deposition, e.g. of a silicon (including polysilicon or monosilicon) or silica film.
• the method comprises partially reducing hexachlorodisilane with a metal hydride compound to give a reaction product comprising pentachlorodisilane.
• Partially reducing hexachlorodisilane with the metal hydride compound generally comprises combining the hexachlorodisilane and the metal hydride compound.
• Combining the hexachlorodisilane and the metal hydride compound may also be referred to as contacting the hexachlorodisilane and the metal hydride compound. Said differently, there is no proactive step required for partial reduction beyond combining the hexachlorodisilane and the metal hydride compound.
• partial reduction refers to but one of the six silicon-bonded chlorine atoms being replaced by or otherwise substituted with a silicon- bonded hydrogen atom, thereby reducing the parent disilane (i.e., hexachlorodisilane) once to give the pentachlorodisilane.
• Partial reduction in the inventive method is limited to but one of the six silicon-bonded chlorine atoms to give the pentachlorodisilane.
• the pentachlorodisilane may be represented by HCl2Si * SiCl3 and/or Cl3Si * SiCl2H.
• the reaction product may also include tetrachlorodisilanes, tnchlorodisilanes, etc.
• the reaction product is purified in the inventive method so as to minimize and/or eliminate such byproducts from the reaction product, thereby giving the purified reaction product comprising the pentachlorodisilane.
• the invention has technical and non-technical advantages.
• One of the problems solved by the processes is providing, relative to conventional processes, improved processes of making the pentachlorodisilane.
• the inventive method typically prepares pentachlorodisilane in higher purity, higher yield, greater selectivity, or a combination of any two or more thereof, than conventional processes.
• the inventive method can be scaled up for high volume production of pentachlorodisilane at low cost, particularly as compared to conventional processes.
• hexachlorodisilane has the formula Cl3SiSiCl3-
• Hexachlorodisilane may be synthesized, prepared, or otherwise obtained.
• hexachlorodisilane may be synthesized via chlorination of calcium silicide (CaSi2).
• Hexachlorodisilane is also commercially available from numerous suppliers.
• the metal hydride compound may comprise any metal hydride compound capable of partially reducing the hexachlorodisilane to give pentachlorodisilane.
• Metal hydride compounds suitable for the purposes of the present invention include, but are not limited to, hydrides of sodium, magnesium, potassium, lithium, boron, calcium, titanium, zirconium, and aluminum, metal hydride compounds including at least one of these same metals, and any combinations thereof.
• the metal hydride compound can be a simple (binary) metal hydride compound or a complex metal hydride compound.
• the metal hydride compound may also include elements, atoms, or substituents other than metal and hydrogen.
• the metal hydride compound may include substituted or unsubstituted hydrocarbyl groups, heteroelements, etc.
• the metal hydride compound is selected from diisobutylaluminum hydride (DIBAH), dimethylaluminum hydride, diethylaluminum hydride, di(n-propyl)aluminum hydride, diisopropylaluminum hydride, di(n-butyl)aluminum hydride, di(sec-butyl)aluminum hydride, di(tert-butyl)aluminum hydride, di(n-pentyl)aluminum hydride, di(iso-pentyl)aluminum hydride, di(sec-pentyl)aluminum hydride, di(3- pentyl)aluminum hydride, di(tert-pentyl)aluminum hydride, di(neo-pentyl)aluminum hydride, isomers of dihexylaluminum hydride, DIBAH), dimethyl
• Vitride, Red-AI, etc. aluminum hydride, lithium hydride, sodium hydride, sodium borohydride, lithium aluminum hydrides (including, for example, LiAI(OtBu)3H or LiAI(iBu)2(OtBu)H, where tBu is tert-butyl and iBu is isobutyl), sodium aluminum hydride, lithium borohydride, magnesium hydride, magnesium borohydride, calcium hydride, titanium hydride, zirconium hydride, tetramethylammonium borohydride, potassium borohydride, etc. Combinations of different metal hydride compounds or combinations of metal hydride compounds with trialkylaluminum compounds may be utilized in concert.
• Any alkyl groups may be independently selected from, for example, methyl, ethyl and isomeric propyl, butyl, pentyl, hexyl, heptyl, octyl, nonyl and/or decyl,
• the metal hydride compound comprises, alternatively consists essentially of, alternatively consists of, diisobutylaluminum hydride (DIBAH).
• DIBAH diisobutylaluminum hydride
• the metal hydride compound is disposed in a carrier vehicle, such as a solvent or dispersant.
• the carrier vehicle may comprise an organic solvent.
• the organic solvent can be an aromatic hydrocarbon such as benzene, toluene, or xylene; an aliphatic hydrocarbon such as heptane, hexane, or octane; a glycol ether such as propylene glycol methyl ether, dipropylene glycol methyl ether, propylene glycol n-butyl ether, propylene glycol n-propyl ether, or ethylene glycol n-butyl ether, a halogenated hydrocarbon such as dichloromethane, 1 ,1 ,1 -trichloroethane or methylene chloride; chloroform; dimethyl sulfoxide; dimethyl formamide, acetonitrile; tetrahydrofuran; white spirits; mineral spirits; nap
• the metal hydride compound When disposed in the carrier vehicle, the metal hydride compound is typically present in the carrier vehicle in an amount to provide from 1 to 99, alternatively from 10 to 80, alternatively from 40 to 60, weight percent based on the combined weight of the metal hydride compound and the carrier vehicle.
• the relative amount of the metal hydride compound utilized may vary dependent upon the particular metal hydride compound selected, the reduction parameters employed, etc.
• the molar ratio of the metal hydride compound to the hexachlorodisilane utilized in the partial reduction influences rates and/or amounts of conversion to, and/or selectivity for, the pentachlorodisilane (i.e., as compared to byproducts).
• the relative amounts of the metal hydride compound and hexachlorodisilane, as well as the molar ratio thereof may vary.
• these relative amounts and the molar ratio are selected to maximize a conversion rate and/or a selectivity of partial reduction of the hexachlorodisilane to pentachlorodisilane.
• using a significant molar excess of the metal hydride compound to the hexachlorodisilane may result in an over reduction of the hexachlorodisilane to byproducts other than pentachlorodisilane (e.g.
• the molar ratio of the hexachlorodisilane to the metal hydride compound is from 1 :0.01 to 1 :3, alternatively from 1 :0.05 to 1 :1 .25, alternatively from 1 :0.1 to 1 :1 .2, alternatively from 1 :0.2 to 1 :1 .1 , alternatively from 1 :0.3 to 1 :1 , alternatively from 1 :0.4 to 1 :0.9, alternatively from 1 :0.5 to 1 :0.8.
• partial reduction of the hexachlorodisilane to prepare the reaction product comprising pentachlorodisilane is carried out in a vessel or reactor.
• the hexachlorodisilane and the metal hydride compound may be fed together or separately to the vessel, or may be disposed in the vessel in any order of addition.
• the vessel or reactor may be heated in any suitable manner, e.g. via a jacket.
• the hexachlorodisilane and the metal hydride compound may be fed to the vessel sequentially over time or at once.
• Parameters may be modified during partial reduction of the hexachlorodisilane to prepare the reaction product comprising pentachlorodisilane.
• temperature, pressure, and other parameters may be independently selected or modified during partial reduction of the hexachlorodisilane to prepare the reaction product comprising pentachlorodisilane.
• Any of these parameters may independently be an ambient parameter (e.g. room temperature and/or atmospheric pressure) and/or a non-ambient parameter (e.g. reduced or elevated temperature and/or reduced or elevated pressure).
• Any parameter may also be dynamic, modified in real time, i.e., during the inventive method, or may be static.
• partial reduction of the hexachlorodisilane to prepare the reaction product comprising pentachlorodisilane is carried out at an elevated temperature.
• the elevated temperature is typically from greater than ambient temperature (e.g. 22-25 °C) to 150, alternatively from 30 to 140, alternatively from 40 to 130, alternatively from 50 to 120, alternatively from 60 to 1 10, alternatively from 70 to 100, alternatively from 75 to 95, alternatively from 80 to 90, °C.
• ambient temperature e.g. 22-25 °C
• 40 to 130 alternatively from 50 to 120, alternatively from 60 to 1 10, alternatively from 70 to 100, alternatively from 75 to 95, alternatively from 80 to 90, °C.
• the hexachlorodisilane and/or the metal hydride compound may be independently heated and combined, combined and heated (prior to, during, and/or after such combination), etc.
• the hexachlorodisilane is heated to the elevated temperature, and the metal hydride compound is combined with the hexachlorodisilane at the elevated temperature.
• the hexachlorodisilane and the metal hydride compound may be combined simultaneously, incrementally, etc.
• the metal hydride compound may be incrementally combined with the hexachlorodisilane compound over time.
• the hexachlorodisilane and the metal hydride compound independently may be stored under an anhydrous condition (i.e., lacking water), under an inert atmosphere, or, typically, both, i.e., an anhydrous inert atmosphere.
• the inert atmosphere is typically a gas comprising molecular nitrogen, helium, argon, or a mixture of any two or more thereof.
• partial reduction of the hexachlorodisilane to prepare the reaction product comprising pentachlorodisilane may be carried out under an anhydrous condition and/or under an inert atmosphere.
• the method may further comprise agitating the hexachlorodisilane and the metal hydride compound.
• the agitating may enhance mixing and contacting together of the hexachlorodisilane and the metal hydride compound when combined, including in a reaction mixture thereof.
• Such contacting independently may use other conditions, with (e.g. concurrently or sequentially) or without (i.e., independent from, alternatively in place of) the agitating.
• the other conditions may be tailored to enhance the contacting, and thus reaction (i.e., partial reduction), of the hexachlorodisilane so as to form the pentachlorodisilane in a particular contacting step.
• Other conditions may be result-effective conditions for enhancing reaction yield or minimizing amount of a particular reaction byproduct included within the reaction product along with the pentachlorodisilane.
• the time during which partial reduction of the hexachlorodisilane to prepare the reaction product comprising pentachlorodisilane is carried out is a function of scale, reaction parameters and conditions, selection of the metal hydride compound, etc.
• the time during which partial reduction of the hexachlorodisilane to prepare the reaction product comprising pentachlorodisilane is carried out is from greater than 0 to 24 hours, alternatively from greater than 0 to 12 hours, alternatively from greater than 0 to 6 hours, alternatively from greater than 0 to 2 hours, after combining the hexachlorodisilane and the metal hydride compound.
• partial reduction of the hexachlorodisilane to prepare the reaction product comprising pentachlorodisilane is carried out in the absence of any carrier vehicle or solvent.
• no carrier vehicle or solvent may be combined discretely with the hexachlorodisilane and/or the metal hydride compound.
• neither the hexachlorodisilane nor the metal hydride compound is disposed in any carrier vehicle or solvent such that no carrier vehicle or solvent is present during partial reduction attributable to the hexachlorodisilane and/or the metal hydride compound.
• partial reduction may be carried out in the presence of a carrier vehicle or solvent.
• a carrier vehicle or solvent Specific examples thereof are introduced above with regard to potential carrier vehicles for the metal hydride compound.
• the reaction product may include various byproducts from partially reducing the hexachlorodisilane. These may include other reduced forms of hexachlorodisilane, e.g. tetrachlorodisilanes, trichlorodisilanes, dichlorodisilanes, etc., residual and/or unreacted amounts of hexachlorodisilane and/or the metal hydride compound, or degradation products thereof.
• the reaction product typically also includes a metal chloride formed from the metal hydride compound upon partial reduction of the hexachlorodisilane. The metal chloride present in the reaction product is generally a function of the metal hydride compound utilized.
• the metal chloride compound may comprise diisobutylaluminum chloride.
• the reaction product typically also includes such carrier vehicle or solvent.
• the method is typically carried out neat, i.e., in the absence of solvent, this is typically not the case.
• the metal chloride is typically a liquid in the reaction product.
• the method further comprises purifying the reaction product to give a purified reaction product comprising the pentachlorodisilane.
• Any suitable technique for purification may be utilized. Examples of suitable techniques include distilling, evaporating, extracting, freeze drying, gas chromatography, ion exchange chromatography, reverse phase liquid chromatography, stripping, and/or volatilizing.
• purifying the reaction product comprises distilling the reaction product to give the purified reaction product.
• distilling the reaction product prepares a crude reaction product comprising the pentachlorodisilane, and the method further comprises purifying the crude reaction product to give the purified reaction product.
• the reaction product may be distilled upon formation such that the crude reaction product is condensed and collected.
• the crude reaction product has a higher content of the pentachlorodisilane than does the reaction product.
• the crude reaction product comprises the pentachlorodisilane in an amount of from 5 to 70, alternatively from 6 to 47, alternatively from 7 to 44, alternatively from 8 to 41 , alternatively from 9 to 38, alternatively from 10 to 35, alternatively from 1 1 to 32, alternatively from 12 to 29, alternatively from 13 to 26, alternatively from 14 to 23, alternatively from 15 to 20, weight percent based on the total weight of the crude reaction product.
• the concentration of the pentachlorodisilane in the crude reaction product may vary from the ranges set forth herein.
• the concentration of the pentachlorodisilane in the crude reaction product may be determined via known methods, e.g. gas chromatography, optionally via a gas chromatography-thermal conductivity detector.
• Distilling the reaction product to prepare the crude reaction product comprising the pentachlorodisilane is typically carried out at (i) an elevated temperature; (ii) a reduced pressure; or (iii) both an elevated temperature and reduced pressure.
• elevated or reduced it is meant as compared to room temperature and atmospheric pressure.
• the number of trays utilized in distillation may be optimized and may influence a concentration or yield of the pentachlorodisilane. For example, use of a greater number of trays via distillation may increase the concentration or yield of the pentachlorodisilane in the crude reaction product.
• the elevated temperature is typically from greater than ambient temperature to 150, alternatively from 30 to 140, alternatively from 40 to 130, alternatively from 50 to 120, alternatively from 60 to 1 10, alternatively from 70 to 100, alternatively from 75 to 95, alternatively from 80 to 90, °C.
• the reduced pressure it typically operated as a vacuum, although any reduced pressure between vacuum and atmospheric pressure may be utilized.
• the reduced pressure may be from greater than 0 to 200, alternatively from greater than 0 to 100, alternatively from greater than 0 to 90, alternatively from greater than 0 to 80, alternatively from greater than 0 to 70, alternatively from greater than 0 to 60, alternatively from greater than 0 to 50, alternatively from greater than 0 to 40, alternatively from greater than 0 to 30, alternatively from greater than 0 to 20, alternatively from 5 to 15, Torr.
• the elevated temperature may also differ from the ranges set forth above, e.g. in the event the reaction product includes any carrier vehicle or solvent.
• the crude reaction product may be condensed and collected at any suitable temperature.
• the crude reaction product is condensed at a temperature of from 0 to 25, alternatively from 0 to 20, alternatively from 0 to 15, alternatively from 0 to 10, alternatively from 4 to 6, °C.
• the crude reaction product may be purified via any suitable technique.
• the purification technique may be the same as or different from the purification technique utilized to prepare the crude reaction product from the reaction product.
• purifying the crude reaction product to give the purified reaction product comprises distilling the crude reaction product.
• purifying the crude reaction product comprises fractionally distilling the crude reaction product. The description below associated with parameters of purifying the crude reaction product apply whether distillation or fractional distillation is utilized.
• distilling the crude reaction product is typically carried out at (i) an elevated temperature; (ii) a reduced pressure; or (iii) both an elevated temperature and reduced pressure.
• elevated or reduced it is meant as compared to room temperature and atmospheric pressure.
• the number of trays utilized in distillation may be optimized and may influence a concentration or yield of the pentachlorodisilane. For example, use of a greater number of trays via distillation may increase the concentration or yield of the pentachlorodisilane.
• the elevated temperature is typically from greater than ambient temperature to 150, alternatively from 30 to 140, alternatively from 40 to 130, alternatively from 50 to 120, alternatively from 60 to 1 10, alternatively from 70 to 100, alternatively from 75 to 95, alternatively from 80 to 90, °C.
• the reduced pressure it typically operated as a vacuum, although any reduced pressure between vacuum and atmospheric pressure may be utilized.
• the reduced pressure may be from greater than 0 to 200, alternatively from greater than 0 to 100, alternatively from greater than 0 to 90, alternatively from greater than 0 to 80, alternatively from greater than 0 to 70, alternatively from greater than 0 to 60, alternatively from greater than 0 to 50, alternatively from greater than 0 to 40, alternatively from greater than 0 to 30, alternatively from greater than 0 to 20, alternatively from 5 to 15, Torr.
• distillation of the crude reaction product utilizes more trays or plates than distillation of the reaction product.
• the number of trays or plates may be modified, and a feed location may also be optimized or modified.
• distillation of the crude reaction product comprises a plurality of purification steps. For example, distillation and/or fractional distillation may be repeated any number of times to further concentrate the pentachlorodisilane in the purified reaction product.
• the purified reaction product refers to the final form of a composition resulting from any number of purification steps to which the reaction product is subjected.
• distillation of the crude reaction product may prepare a first concentrated reaction product.
• Distillation of the first concentrated reaction product may then prepare a second concentrated reaction product.
• Distillation of the second concentrated reaction product may then prepare a third concentrated reaction product.
• Each iteration of the reaction product is distinguished from the prior iteration (i.e., the third concentrated reaction product is distinguished from the second concentrated reaction product, and the second concentrated reaction product is distinguished from the first concentrated reaction product) by virtue of a relative concentration of the pentachlorodisilane in a particular concentrated reaction product, as compared to other components (e.g. byproducts, starting materials, etc.) therein.
• the relative concentration of the pentachlorodisilane i.e., the purity
• Each iterative purification step may be independently selected.
• the first concentrated reaction product comprises the pentachlorodisilane in an amount of from 20 to 83, alternatively from 22 to 80, alternatively from 24 to 77, alternatively from 26 to 74, alternatively from 28 to 71 , alternatively from 30 to 68, alternatively from 32 to 65, alternatively from 34 to 62, alternatively from 36 to 59, alternatively from 38 to 56, alternatively from 40 to 53, alternatively from 42 to 50, weight percent based on the total weight of the first concentrated reaction product.
• the concentration of the pentachlorodisilane in the first concentrated reaction product may vary from the ranges set forth herein.
• distillation of the crude reaction product could involve additional trays or plates could be utilized in an effort to provide further purification in a single purification step.
• the concentration of the pentachlorodisilane in the first concentrated reaction product may be determined via known methods, e.g. gas chromatography, optionally via a gas chromatography-thermal conductivity detector.
• each iterative purification step may be independently selected, in certain embodiments, each iterative purification step comprises distillation. Even in this embodiments, parameters associated with distillation (e.g. the elevated temperature and/or the reduced pressure) may be independently selected via each iterative distillation step. Typically, however, each iterative distillation step utilizes the parameters identified above relative to the elevated temperature and the reduced pressure.
• the method comprises at least 1 , alternatively at least 2, alternatively 3, iterative distillation steps subsequent to preparing the crude reaction product comprising the pentachlorodisilane to give the purified reaction product comprising the pentachlorodisilane.
• the method is not so limited, any number of iterative distillation steps, or iterative purification steps, may be utilized. The number of iterative distillation steps, or iterative purification steps, is typically contingent on a desired concentration of the pentachlorodisilane in the purified reaction product.
• Any number of individual reaction products, crude reaction products, or concentrated reaction products may be combined to form a batch.
• a number of independently prepared crude reaction products are combined to form a batch of crude reaction product.
• the batch of crude reaction product is then purified according to the present method to give the pentachlorodisilane.
• the purified reaction product comprises the pentachlorodisilane in an amount of at least 50, alternatively at least 55, alternatively at least 60, alternatively at least 65, alternatively at least 70, alternatively at least 75, alternatively at least 80, alternatively at least 81 , alternatively at least 82, alternatively at least 83, alternatively at least 84, alternatively at least 85, alternatively at least 86, alternatively at least 87, alternatively at least 88, alternatively at least 89, alternatively at least 90, alternatively at least 91 , alternatively at least 92, alternatively at least 93, alternatively at least 94, alternatively at least 95, alternatively at least 96, alternatively at least 97, alternatively at least 97.5, alternatively at least 98, wt.
• the concentration of the pentachlorodisilane in the purified reaction product may be 100, alternatively 99.9999999, alternatively 99.999999, alternatively 99.99999, alternatively 99.9999, alternatively 99.999, alternatively 99.99, alternatively 99.9, alternatively 99.0, wt.%.
• the purified reaction product comprises aluminum in an amount of less than 50 parts per billion (ppb).
• ranges and subranges sufficiently describe and enable various embodiments of the present invention, and such ranges and subranges may be further delineated into relevant halves, thirds, quarters, fifths, and so on.
• a range "of from 0.1 to 0.9" may be further delineated into a lower third, i.e., from 0.1 to 0.3, a middle third, i.e., from 0.4 to 0.6, and an upper third, i.e., from 0.7 to 0.9, which individually and collectively are within the scope of the appended claims, and may be relied upon individually and/or collectively and provide adequate support for specific embodiments within the scope of the appended claims.
• a range such as "at least,”
• a range of “at least 10” inherently includes a subrange of from at least 10 to 35, a subrange of from at least 10 to 25, a subrange of from 25 to 35, and so on, and each subrange may be relied upon individually and/or collectively and provides adequate support for specific embodiments within the scope of the appended claims.
• an individual number within a disclosed range may be relied upon and provides adequate support for specific embodiments within the scope of the appended claims.
• a range "of from 1 to 9" includes various individual integers, such as 3, as well as individual numbers including a decimal point (or fraction), such as 4.1 , which may be relied upon and provide adequate support for specific embodiments within the scope of the appended claims.
• Hexachlorodisilane (3.48 kg; 12.9 mol) is loaded into a 12 L jacketed reactor and then heated to and held at a temperature of 80 °C. The contents of the reactor is then maintained at a temperature between 80-90 °C and agitated while a metal hydride compound (DIBAH; 1 .48 kg; 10.4 mol) is added over a period of 2 hours to give a reaction mixture.
• DIBAH metal hydride compound
• the reaction mixture is agitated for 30 minutes in the reactor and then distilled through a 5-tray column under vacuum to give a reaction product comprising pentachlorodisilane (PCDS) (-3.2 kg; 16 % PCDS via GC-TCD integrations), which is then condensed through a cooled condenser (5 °C) and collected in a 3 L receiving flask.
• PCDS pentachlorodisilane
• the reaction product is then fractionally distilled under vacuum (down to 10 Torr) at 80 °C pot temperature through a 20-tray column to give a crude reaction product comprising pentachlorodisilane (PCDS) (494 g; 46 % PCDS via GC-TCD integrations).

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• 2018
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